CN106732436A - A kind of magnetic starch compound adsorbent preparation method and application - Google Patents
A kind of magnetic starch compound adsorbent preparation method and application Download PDFInfo
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- CN106732436A CN106732436A CN201710081457.3A CN201710081457A CN106732436A CN 106732436 A CN106732436 A CN 106732436A CN 201710081457 A CN201710081457 A CN 201710081457A CN 106732436 A CN106732436 A CN 106732436A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/24—Naturally occurring macromolecular compounds, e.g. humic acids or their derivatives
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28002—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their physical properties
- B01J20/28009—Magnetic properties
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/286—Treatment of water, waste water, or sewage by sorption using natural organic sorbents or derivatives thereof
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4812—Sorbents characterised by the starting material used for their preparation the starting material being of organic character
- B01J2220/4825—Polysaccharides or cellulose materials, e.g. starch, chitin, sawdust, wood, straw, cotton
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/308—Dyes; Colorants; Fluorescent agents
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Abstract
The invention discloses a kind of methods and applications for preparing magnetic starch adsorption agent, the preparation method is：1 vinyl imidazole and monoxone are mixed by a certain percentage, cationic liquid is prepared, obtain solid clean drying after add potassium peroxydisulfate make initiator polymerization obtain poly ion liquid.Poly ion liquid and starch are mixed to form suspension, stirring makes to add Fe after it is well mixed3O4Nano-particle, poly ion liquid, starch and Fe3O4By certain mass than mixing.The mixture for obtaining finally is obtained magnetic starch compound adsorbent by being dried again after freeze-drying.The inventive method has low cost, easily-controlled reaction conditions, consume energy low advantage, and the magnetic adsorbent for preparing has the advantages that adsorption high, good dispersion, easily separated.The magnetic starch adsorption agent can be applied to process heavy metal ion and dyestuff in sewage.Therefore there is good application prospect at aspects such as sewage disposal, separation sciences.
Description
Technical field
The present invention relates to environment remediation field of new technical field, a kind of specifically magnetic starch compound adsorbent
Preparation method and application.
Background technology
In recent years, with the development of fast industrialization, the sewage containing dyestuff and heavy metal brings very big to environment
Burden, while the heavy metal chromium ion dissolved in waste water and dyestuff are enriched with by various biological chains in water body, finally by aquatic products
Enter human body via food chain, cause rhinorrhea, sneeze, itch, nosebleed etc., make when serious human recycle system's exhaustion to
Health brings serious influence.It is not only harmful to human health, ecology is had an effect on, economic, politics etc..Therefore, go
Heavy metal ion and dyestuff in water removal have turned into problem demanding prompt solution, in the urgent need to finding low-carbon (LC), economical and simple side
Method improves the contaminated wastewater of presence.Process heavy metal ions in wastewater method mainly have chemical precipitation method, oxidation-reduction method,
Ion-exchange, electrolysis, membrane separation process etc., but the price of these methods is all very expensive, also brings along secondary pollution.Wherein
Absorption method is easy due to operating method, and treatment effect is more satisfactory, has become the water body that heavy-metal ion removal and dyestuff cause
One of main method of pollution, it is it is critical that the adsorbent of selection efficient green.
The content of the invention
In view of the shortcomings of the prior art, the present invention provide it is a kind of based on process is simple, low cost, easily obtain and can magnetic point
From the preparation method of the novel magnetic composite of regeneration, there is efficient, energy-conservation, environmental protection, the composite wood
Material has the feature of the dyestuff and heavy metal ion that remove polluted-water simultaneously.
To achieve the above object, the technical solution adopted by the present invention is：A kind of magnetic starch compound adsorbent preparation method,
Step includes：
(1) preparation of poly ion liquid
1- vinyl imidazoles and monoxone are with mol ratio 1：1~4 ratio mixes, and is reacted in 100mL round-bottomed flasks, with
50mL acetonitriles as solvent, in N2Under the conditions of be heated to 70~90 DEG C stirring 24h, washed with acetonitrile after cooling, in 70 DEG C of conditions
Under dry to obtain white solid, as ionic liquid；
5g ionic liquids are weighed, 5mL water dissolves solids are added, a certain amount of potassium peroxydisulfate is added, in 90~110 DEG C of N2Bar
Part reacts 8h, and water is removed after cooling, is finally washed 3 times with ethyl acetate, and 80 DEG C of drying obtain poly ion liquid in vacuum drying chamber；
(2) poly ion liquid, starch and Fe3O4The preparation of composite
Poly ion liquid and starch are 1 in mass ratio:1~8 ratio is added in round-bottomed flask, is reacted under the conditions of 90 DEG C
It is well mixed it after 0.5h, 1.56g Fe is then added in mixed solution3O4, temperature be raised to 65 DEG C reaction 24h, reaction knot
Being poured into after beam in mould makes its thickness less than 1cm, is freezed 24 hours in refrigerator, and the sample after freezing carries out freeze-drying, freezing
After drying in vacuum drying chamber 80 DEG C dry 2h, then heat up 105 DEG C dry 2h, finally dried at 130 DEG C 1.5h obtain magnetic answer
Close adsorbent.
Further, in step (1), the 1- vinyl imidazoles and monoxone are with mol ratio 1:1~3.
Further, in step (1), the N2Under the conditions of be heated to 75~90 DEG C.
Further, in step (1), the potassium peroxydisulfate addition is the 1~3% of ionic liquid.
Further, in step (2), the poly ion liquid and starch quality ratio are 1:1~7.
Further, the poly ion liquid and starch quality ratio are 1:1~5.
The present invention also provides a kind of magnetic starch compound adsorbent and its application in sewage disposal.
The method have the benefit that：It is raw material that the present invention uses starch, and starch is that one kind is nontoxic, inexpensively
It is easy to get, the polysaccharide biomaterial of green environment is widely used in the industries such as food, papermaking, medicine, oil.In starch structure
There is great amount of hydroxy group group to provide good carrier for the modified of starch, original some physics of starch are changed via modified starch
Chemical property is so as to more meet human wants.The invention provides the preparation method of modified starch adsorbent, work(is prepared for
Magnetic starch can be changed, and utilize magnetic starch heavy-metal ion removal and dyestuff.Modified magnetic starch adsorption agent is compared with starch
It is the comparatively ideal porous adsorbing material of a class with some homogeneous holes with high adsorption capacity, adds magnetic property using extraneous
Magnetic field reaches quick Magneto separate.
Brief description of the drawings
In order to illustrate more clearly about the embodiment of the present invention or technical scheme of the prior art, below will be to embodiment or existing
The accompanying drawing to be used needed for having technology description is briefly described, it should be apparent that, drawings in the following description are only this
Some embodiments of invention, for those of ordinary skill in the art, without having to pay creative labor, may be used also
Other accompanying drawings are obtained with according to these accompanying drawings.
Fig. 1 is the influence that pH value of solution is adsorbed to Cr VI；
Fig. 2 is Adsorption Effect of the quantity of sorbent to Cr VI；
Fig. 3 is influence of the time to the absorption of Cr VI；
Fig. 4 is 25 DEG C of Adsorption Effects to Cr VI of temperature；
Fig. 5 is influence of the coexisting ion to Cr VI adsorption effect；
Fig. 6 is the influence under pH value of solution to orange (II) adsorption effect；
Fig. 7 is influence of the quantity of sorbent to orange (II) adsorption effect；
Fig. 8 is influence of the adsorption time to orange (II) adsorption effect；
Fig. 9 is 25 DEG C of influences to orange (II) adsorption effect of temperature；
Figure 10 is test NaCl, Na2SO4、Na3PO4PH value in the presence of three kinds of ions；
Figure 11 is influence of the coexisting ion to Cr VI adsorption effect；
Figure 12 is magnetic starch compound adsorbent B-H loop and adsorbing separation photo.
Specific embodiment
Below in conjunction with the accompanying drawing in the embodiment of the present invention, the technical scheme in the embodiment of the present invention is carried out clear, complete
Site preparation is described, it is clear that described embodiment is only a part of embodiment of the invention, rather than whole embodiments.It is based on
Embodiment in the present invention, it is every other that those of ordinary skill in the art are obtained under the premise of creative work is not made
Embodiment, belongs to the scope of protection of the invention.
1- vinyl imidazoles, monoxone, potassium peroxydisulfate, orange (II) Fe in embodiment3O4Purchased from the Aladdin limited public affairs of chemistry
Department；Ethyl acetate, acetonitrile, sodium chloride, sodium sulphate, sodium phosphate are purchased from agrochemicals chemical reagent work of Chengdu section；Starch is purchased from Sichuan friend
Good Food Co., Ltd.
Embodiment 1
A kind of novel magnetic starch compound adsorbent preparation method, step includes：
(1) preparation of poly ion liquid
1- vinyl imidazoles and monoxone are with mol ratio 1：1 ratio mixes, and is reacted in 100mL round-bottomed flasks, with 50mL
Acetonitrile as solvent, in N2Under the conditions of be heated to 70 DEG C stirring 24h, washed with acetonitrile after cooling, dried under the conditions of 70 DEG C
To white solid, and it is ionic liquid；
5g ionic liquids are weighed, 5mL water dissolves solids are added, the potassium peroxydisulfate of ionic liquid 1% is added, in N2Condition
Under be heated to 90 DEG C stirring 8h, water is removed after cooling, finally 3 ethyl acetate are washed with ethyl acetate, finally in vacuum drying chamber
In 80 DEG C of drying obtain poly ion liquid；
(2) poly ion liquid, starch and Fe3O4The preparation of composite
Poly ion liquid and starch are 1 in mass ratio:1 ratio is added in round-bottomed flask, and 0.5h is reacted under the conditions of 90 DEG C
After be well mixed it, 1.56g Fe are then added in mixed solution3O4, temperature is raised to 65 DEG C of reaction 24h, after reaction terminates
Pouring into mould makes its thickness less than 1cm, is freezed 24 hours in refrigerator, and the sample after freezing carries out freeze-drying, freeze-drying
Afterwards in vacuum drying chamber 80 DEG C dry 2h, then heat up 105 DEG C of re-dry 2h, finally dried at 130 DEG C 1.5h obtain magnetic answer
Close adsorbent.
Embodiment 2
A kind of novel magnetic starch compound adsorbent preparation method, step includes：
(1) preparation of poly ion liquid
1- vinyl imidazoles and monoxone are with mol ratio 1：2 ratios mix as round-bottomed flask in, using 50mL acetonitriles as
Solvent, in N2Under the conditions of be heated to 75 DEG C stirring 24h, wash with acetonitrile after cooling, under the conditions of 70 DEG C drying obtain white consolidate
Body, and be ionic liquid；
The potassium peroxydisulfate of 5g ionic liquids, addition 5mL water dissolves solids, then ionic liquid 2% is weighed, in N2Under the conditions of plus
Heat removes water to 100 DEG C of stirring 8h after cooling, finally 3 ethyl acetate are washed with ethyl acetate, finally 80 in vacuum drying chamber
DEG C drying obtains poly ion liquid；
(2) poly ion liquid, starch and Fe3O4The preparation of composite
Poly ion liquid and starch are 1 in mass ratio:4 ratios are added in round-bottomed flask, and 0.5h is reacted under the conditions of 90 DEG C
After be well mixed it, 1.56g Fe are then added in mixed solution3O4, temperature is raised to 65 DEG C of reaction 24h, after reaction terminates
Pouring into mould makes its thickness less than 1cm, is freezed 24 hours in refrigerator, and the sample after freezing carries out freeze-drying, freeze-drying
Afterwards in vacuum drying chamber 80 DEG C dry 2h, then heat up 105 DEG C of re-dry 2h, finally dried at 130 DEG C 1.5h obtain magnetic answer
Close adsorbent.
Embodiment 3
A kind of novel magnetic starch compound adsorbent preparation method, step includes：
(1) preparation of poly ion liquid
1- vinyl imidazoles and monoxone are with mol ratio 1：3 ratios mix as round-bottomed flask in, using 50mL acetonitriles as
Solvent, in N2Under the conditions of be heated to 80 DEG C stirring 24h, wash with acetonitrile after cooling, under the conditions of 70 DEG C drying obtain white consolidate
Body, and be ionic liquid；
5g ionic liquids are weighed, 5mL water dissolves solids are added, the potassium peroxydisulfate of ionic liquid 3% is added, in N2Condition
Under be heated to 90~110 DEG C of stirring 8h, water is removed after cooling, finally wash 3 ethyl acetate with ethyl acetate, it is finally dry in vacuum
80 DEG C of drying obtain poly ion liquid in dry case；
(2) poly ion liquid, starch and Fe3O4The preparation of composite
Poly ion liquid and starch are 1 in mass ratio:6 ratios are added in round-bottomed flask, and 0.5h is reacted under the conditions of 90 DEG C
After be well mixed it, 1.56g Fe are then added in mixed solution3O4, temperature is raised to 65 DEG C of reaction 24h, after reaction terminates
Pouring into mould makes its thickness less than 1cm, is freezed 24 hours in refrigerator, and the sample after freezing carries out freeze-drying, freeze-drying
Afterwards in vacuum drying chamber 80 DEG C dry 2h, then heat up 105 DEG C of re-dry 2h, finally dried at 130 DEG C 1.5h obtain magnetic answer
Close adsorbent.
Embodiment 4
Suction-operated of the magnetic composite to Cr (VI)
Weigh 5mg magnetic composite PIL-St@Fe3O4It is added in the solution that 50mL Cr (VI) concentration is 20mg/L,
System pH=1.72 is reconciled with hydrochloric acid.Adsorb 2h under the conditions of 25 DEG C, it is to be adsorbed reach saturation after magnetic point is carried out with additional magnet
From, take separate after supernatant the dense of its remaining Cr (VI) is surveyed with 723 spectrophotometers by developer of diphenyl kappa trap
Degree, the adsorbance of maximum is calculated further according to formula, is as a result shown：68.9mg/g (Fig. 3).
Embodiment 5
PIL-St@Fe3O4Suction-operated of the magnetic composite to orange (II)
Weigh 5mg magnetic composites to be added in the solution that orange (II) concentration of 50mL is 50mg/L, under the conditions of 25 DEG C
Absorption 2h, it is to be adsorbed reach saturation after carry out Magneto separate with additional magnet, take separate after 723 spectrophotometers of supernatant
To survey the concentration of its residue orange (II), the adsorbance of maximum is calculated further according to formula, as a result shown：489.8mg/g (figures
8)。
Fig. 1 is influences of the pH to the absorption of Cr VI.Influences of the bright pH of the chart to Cr (VI) adsorption effect.PH is to Cr
(VI) adsorbance has a great impact, and modified starch adsorbent is reduced to the clearance of Cr (VI) with the rising of pH.Low pH bars
Adsorption efficiency high is primarily due to protonation and the positively charged electrostatic attraction to cause Cr (VI) ion under part.With the increasing of pH
Big adsorbance reduces the N because in the protonation and adsorbent of (=N -) on PIL+, secondly absorption high under low ph condition
Efficiency is because HCrO4 -Negative electrical charge and PIL on positive charge electrostatic attraction.Additionally, also there is suction-operated appearing on PIL
Cl–And HCrO4 -Ion exchange；At lower ph, there is substantial amounts of H3O+, pH increase also there is OH-And CrO4 2-。
Fig. 2 is Adsorption Effect of the quantity of sorbent to Cr VI.The bright adsorbance of the chart subtracts with the increase of quantity of sorbent
Few, quantity of sorbent is reduced, and Cr (VI) can take up effective adsorption site, and the adsorbance for calculating is big because adsorbent mass
It is small.When quantity of sorbent is low, the concentration of Cr (VI) be it is constant, the surface area of adsorbent may be insufficient to make Cr (VI) from
Son is adsorbed.Do not have adsorbable chromium to deposit in the solution, the removal efficiency of Cr (VI) is just reduced.
As the increase of quantity of sorbent, adsorption site and surface area are increased in figure, the removal efficiency increase of Cr (VI) can
It is that the adsorbance calculated by formula reduces on the contrary.In the starting stage, adsorbance increases because there is the absorption table of abundance
Area, the passage avtive spot of time is reduced, and reaches balance.
Fig. 3 is Adsorption Effect of the different time to Cr VI.The bright 60min in the time of the chart reaches balance, starts rank
Section is relatively fast because of many rates of adsorption of adsorption site.
It in temperature is 25 DEG C of Adsorption Effects to Cr VI that Fig. 4 is.Non-linear simulation is carried out to it, more meets not human relations Delhi
Uncommon isothermal adsorption.
Fig. 5 is the influence to Cr VI adsorption effect under coexisting ion.Showing to have the presence of heterogeneous ion can change liquid
Mutually chemistry, has metal electric double layer in adsorbent surface.Na2SO4、Na3PO4Influence is very big, from 0-0.2 so that the absorption of Cr (VI)
Loss in efficiency is very big, and reason is SO4 2-And PO4 3-Compare Cl-Institute is electrically charged more, can occupy the adsorption site of adsorbent, occupied
Site can reduce surface charge and then the Coulomb repulsion of surface and Cr (VI) can be increased.
Fig. 6 is the influence to orange (II) adsorption effect under different pH.C will become apparent from being adsorbed with the increase of pH from figure
Amount reduces.Adsorbent removal is orange very big dependence to pH, the surface charge of the pH influence adsorbents of solution and dyestuff
Degree of ionization.
As pH increase adsorbances reduce, it is the interaction due to electrostatic this result occur.Maximal absorptive capacity is appeared in
PH=1.72, because orange (II) deprotonation has the electrostatic attraction of positive charge in PIL in negative electrical charge and adsorbent.With pH
Increase, negatively charged surface and anionic dye orange (II) intermolecular Coulomb repulsion increases, and adsorbance reduces therewith.
Fig. 7 is influence of the adsorption time to orange (II) adsorption effect.Starting stage adsorbent adsorption site is more, absorption
Speed is relatively fast.With occupying for site, the rate of adsorption becomes slow.Finally slowly reach adsorption equilibrium.
Fig. 8 adsorbances are changed with time, and balance is reached when 2h.
Fig. 9 be temperature be 25 DEG C of influences to orange (II) adsorption effect.Non-linear simulation is carried out to it, more meets bright
Miao Er isotherm adsorption models.
Figure 10 is test NaCl, Na2SO4、Na3PO4PH value in the presence of three kinds of ions.
Figure 11 is magnetic PIL-St@Fe3O4To the influence of Cr VI adsorption effect under composite coexisting ion.Only study
NaCl and Na2SO4Two kinds of ions are because orange (II) color change interval is：7.4 (amber)~8.6 (orange), 10.2 (orange)
~11.8 (red).Due to Na3PO4PH>11.8, orange (II) is changed into red, cannot just consider Na3PO4In the presence of it is right
In the influence of orange (II) adsorbance.
Figure 12 is magnetic PIL-St@Fe3O4Composite arrives the B-H loop of 10kOe, saturation magnetic in magnetic field range -10kOe
Change value is 0.056, and disclosing sample has excellent magnetic.In addition, being also carried out PIL-St@Fe3O4The Magneto separate test of sample, then
Under externally-applied magnetic field Magneto separate phenomenon clearly, discovery be placed in the vial near magnet sample can with the short time in
Separate.
Those skilled in the art of the present technique are appreciated that unless otherwise defined, all terms used herein (including technology art
Language and scientific terminology) have with art of the present invention in those of ordinary skill general understanding identical meaning.Should also
Understand, those terms defined in such as general dictionary should be understood that the meaning having with the context of prior art
The consistent meaning of justice, and unless defined as here, will not be with idealizing or excessively formal implication be explained.
It should be noted last that：Above example is only used to illustrative and not limiting technical scheme, although ginseng
The present invention has been described in detail according to above-described embodiment, it will be apparent to an ordinarily skilled person in the art that：Still can be to this
Invention is modified or equivalent, any modification or partial replacement without departing from the spirit and scope of the present invention, and its is equal
Should cover in the middle of scope of the presently claimed invention.
Claims (8)
1. a kind of magnetic starch compound adsorbent preparation method, it is characterised in that step includes：
(1) preparation of poly ion liquid
1- vinyl imidazoles and monoxone are with mol ratio 1：1~4 ratio mixes, and is reacted in 100mL round-bottomed flasks, with 50mL second
Nitrile as solvent, in N2Under the conditions of be heated to 70~90 DEG C stirring 24h, wash with acetonitrile after cooling, under the conditions of 70 DEG C drying
Obtain white solid, as ionic liquid；
5g ionic liquids are weighed, 5mL water dissolves solids are added, a certain amount of potassium peroxydisulfate is added, in 90~110 DEG C of N2Condition is anti-
8h is answered, water is removed after cooling, finally washed 3 times with ethyl acetate, 80 DEG C of drying obtain poly ion liquid in vacuum drying chamber；
(2) poly ion liquid, starch and Fe3O4The preparation of composite
Poly ion liquid and starch are 1 in mass ratio:1~8 ratio is added in round-bottomed flask, after reacting 0.5h under the conditions of 90 DEG C
It is well mixed, 1.56g Fe are then added in mixed solution3O4, temperature be raised to 65 DEG C reaction 24h, reaction terminate after fall
To enter make in mould its thickness less than 1cm, freezed 24 hours in refrigerator, the sample after freezing carries out freeze-drying, after freeze-drying
In vacuum drying chamber, 80 DEG C dry 2h, and then heating up 105 DEG C dries 2h, 1.5h is finally dried at 130 DEG C and obtains magnetic coupling absorption
Agent.
2. magnetic starch compound adsorbent preparation method according to claim 1, it is characterised in that in step (1), the 1-
Vinyl imidazole and monoxone are with mol ratio 1:1~4.
3. magnetic starch compound adsorbent preparation method according to claim 1, it is characterised in that in step (1), the N2
Under the conditions of be heated to 70~90 DEG C.
4. magnetic starch compound adsorbent preparation method according to claim 1, it is characterised in that in step (1), the mistake
Potassium sulfate addition is the 1~3% of ionic liquid.
5. magnetic starch compound adsorbent preparation method according to claim 1, it is characterised in that described poly- in step (2)
Ionic liquid and starch quality ratio are 1:1~8.
6. magnetic starch compound adsorbent preparation method according to claim 5, it is characterised in that the poly ion liquid and
Starch quality ratio is 1:1~7.
7. the magnetic starch compound adsorbent for being prepared according to any one of claim 1~6 methods described.
8. application of the magnetic starch compound adsorbent in sewage disposal according to claim 7.
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103265492A (en) * | 2013-05-16 | 2013-08-28 | 西北工业大学 | Chlorinated 1-vinyl-3-carboxymethyl imidazole polymerizable acidic ionic liquid and synthetic method thereof |
| CN103980424A (en) * | 2014-05-08 | 2014-08-13 | 嘉兴学院 | Graphene-poly ionic liquid composite material, and preparation method and application thereof |
| CN105087542A (en) * | 2015-09-17 | 2015-11-25 | 李爱冰 | Environmental stress sensitive type immobilized enzyme porous micro-sphere carrier material and preparing method of porous micro-sphere carrier material |
| CN105126780A (en) * | 2015-07-29 | 2015-12-09 | 厦门大学 | Polyion liquid-based chelated absorbent and preparation method thereof |
| US20160032493A1 (en) * | 2014-08-01 | 2016-02-04 | Taiwan Textile Research Institute | Preparation method of polysaccharide fiber |
| CN105964306A (en) * | 2016-05-03 | 2016-09-28 | 河南师范大学 | Poly(ionic liquid)-based magnetic nanoparticle and its preparation method and use in three-ingredient reaction |
-
2017
- 2017-02-15 CN CN201710081457.3A patent/CN106732436B/en not_active Expired - Fee Related
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103265492A (en) * | 2013-05-16 | 2013-08-28 | 西北工业大学 | Chlorinated 1-vinyl-3-carboxymethyl imidazole polymerizable acidic ionic liquid and synthetic method thereof |
| CN103980424A (en) * | 2014-05-08 | 2014-08-13 | 嘉兴学院 | Graphene-poly ionic liquid composite material, and preparation method and application thereof |
| US20160032493A1 (en) * | 2014-08-01 | 2016-02-04 | Taiwan Textile Research Institute | Preparation method of polysaccharide fiber |
| CN105126780A (en) * | 2015-07-29 | 2015-12-09 | 厦门大学 | Polyion liquid-based chelated absorbent and preparation method thereof |
| CN105087542A (en) * | 2015-09-17 | 2015-11-25 | 李爱冰 | Environmental stress sensitive type immobilized enzyme porous micro-sphere carrier material and preparing method of porous micro-sphere carrier material |
| CN105964306A (en) * | 2016-05-03 | 2016-09-28 | 河南师范大学 | Poly(ionic liquid)-based magnetic nanoparticle and its preparation method and use in three-ingredient reaction |
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| CN110652969B (en) * | 2019-09-29 | 2022-03-11 | 陕西科技大学 | Preparation method of polyion liquid modified dialdehyde starch film as adsorbing material |
| CN112439389A (en) * | 2020-10-30 | 2021-03-05 | 广西大学 | Magnetic starch bentonite wastewater treatment agent and preparation method thereof |
| CN113368841A (en) * | 2021-06-12 | 2021-09-10 | 中国科学院青岛生物能源与过程研究所 | Method for preparing magnetic multi-effect adsorbent by utilizing enzymolysis residues through dry method |
| CN113368841B (en) * | 2021-06-12 | 2022-07-01 | 中国科学院青岛生物能源与过程研究所 | Method for preparing magnetic multi-effect adsorbent by utilizing enzymolysis residues through dry method |
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